CN110368968B - NiFe-LDH/Ti3C2/Bi2WO6Nano-sheet array and preparation method and application thereof - Google Patents
NiFe-LDH/Ti3C2/Bi2WO6Nano-sheet array and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B01J35/33—
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- B01J35/39—
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- B01J35/61—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention provides a NiFe-LDH/Ti3C2/Bi2WO6A nano-sheet array, a preparation method and application thereof. The preparation method comprises the following steps: growing Ti with regular appearance on a conductive substrate by adopting a solvothermal method3C2/Bi2WO6A nanosheet array; by electrochemical deposition on Ti3C2/Bi2WO6Depositing NiFe-LDH on the surface of the nano sheet array to obtain NiFe-LDH/Ti3C2/Bi2WO6A nanosheet array. The nanosheet array can be used as a photocatalyst to be applied to photocatalytic reaction, as a photoelectrode to be applied to photoelectric catalytic reaction or as a photoelectric conversion device to be applied to photoelectric devices and solar cells, and has a good catalytic effect.
Description
Technical Field
The invention relates to a preparation method of a nanosheet array, in particular to a NiFe-LDH/Ti3C2/Bi2WO6A preparation method of a nanosheet array belongs to the technical field of material preparation.
Background
In recent decades, with the rapid development of industry and economy, great convenience is brought to human beings, but at the same time, serious environmental pollution problems are caused, wherein the problem of water pollution is particularly serious. The photocatalysis technology is a green and environment-friendly technology which is rapidly developed in recent decades and can directly utilize solar energy to convert organic pollutant ores into water and carbon dioxide.
Bi2WO6The advantages of no toxicity, high stability, multiple active sites, visible light response, low price and easy acquisition are widely researched. Bi2WO6The crystal is composed of [ Bi2O2]2+Layer and (WO)4)2-The layers are alternately stacked, and the unique layered structure is beneficial to the migration of photo-generated charges in the photocatalysis process, so that the photocatalysis performance is improved. And powder Bi2WO6And Bi of particle composition2WO6Film phase ratio, Bi2WO6The nanosheet array has the advantages of higher specific surface area, better light capturing performance, more reactive sites, easiness in recycling and reusing and the like, however, pure Bi2WO6The higher probability of the photogenerated electron-hole recombination of the material still cannot meet the requirement of practical application, and an effective improvement method needs to be explored to reduce the recombination probability of photogenerated charges.
At present, the Bi is improved mainly by methods such as noble metal deposition, quantum dot sensitization, compounding with other semiconductors, surface modification and the like2WO6The photocatalytic efficiency of (c). However, these modification methods are basically limited to Bi2WO6Powder of Bi2WO6The research on the thin film is little, so that the composite Bi with close contact, good stability and excellent charge separation capability is constructed2WO6The research of the film has important significance.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a composite Bi with high photocatalytic efficiency2WO6Preparation method of nanosheet array film and composite Bi obtained by preparation method2WO6The nanosheet array film is good in stability and excellent in charge separation capability.
In order to achieve the technical purpose, the invention provides NiFe-LDH/Ti3C2/Bi2WO6A method for preparing a nanoplate array, the method comprising the steps of:
dipping a conductive substrate into Ti3C2/Bi2WO6In the precursor solution, carrying out solvothermal reaction to grow Ti with regular shape on the conductive substrate3C2/Bi2WO6A nanosheet array;
by electrochemical deposition on Ti3C2/Bi2WO6Depositing NiFe-LDH on the nano sheet array, rinsing and naturally oxidizing to obtain NiFe-LDH/Ti3C2/Bi2WO6A nanosheet array.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The preparation method of the nanosheet array adopts a solvothermal method to directly grow Ti with regular shape on a conductive substrate3C2/Bi2WO6Nano sheet array, depositing NiFe-LDH on the surface of the nano sheet array by electrochemical deposition method, and NiFe-LDH/Ti prepared by the method3C2/Bi2WO6The ternary composite nanosheet array exposes a large proportion of a {001} crystal face, and has good photoelectrocatalytic degradation performance.
NiFe-LDH/Ti obtained by the preparation method of the invention3C2/Bi2WO6The ternary composite nanosheet array can be used as a photocatalyst to be applied to photocatalytic reaction, or used as a photoelectric conversion device to be applied to photoelectric flexible devices and solar cells, and is particularly applied to photocatalytic degradation of pollutants.
The preparation method of the invention comprises the preparation of Ti3C2And (5) powder preparation. Wherein, Ti3C2The powder is prepared by the following steps:
mixing Ti3AlC2Mixing the powder with HF solution, stirring at room temperature for 48-96 h, and etching to remove Ti3AlC2The Al layer in the alloy is Ti3C2(ii) a Wherein, Ti3AlC2The mass ratio of the powder to HF is 1: (5-30);
after centrifugal washingAir-drying to obtain Ti3C2And (3) powder.
In one embodiment of the present invention, Ti is prepared3C2In the case of powder, the HF solution is used in a concentration of 40wt% to 99 wt%.
In one embodiment of the present invention, Ti is prepared3C2When powder is used, the rotation speed of centrifugal washing is 5000r/min-10000 r/min; the times of centrifugal washing are 4-8 times; the time of each centrifugation is 5min-30 min.
In one embodiment of the present invention, Ti is prepared3C2When the powder is prepared, the vacuum drying temperature is 50-100 ℃; the vacuum drying time is 12-48 h.
The preparation method of the invention comprises the preparation of Ti3C2/Bi2WO6And (5) precursor solution.
Wherein Ti is prepared3C2/Bi2WO6The precursor solution comprises the following steps:
adding Na to the ethylene glycol solution of PVP2WO4·2H2O, obtaining a mixed solution I; wherein the mass ratio of the volume of the ethylene glycol to the PVP is (10-90) mL: (0.5-2.5) g; na (Na)2WO4·2H2The mass ratio of O to PVP is 1: (1-5);
adding Ti to a solution of PVP in ethylene glycol3C2Powder of Bi (NO) and re-dissolved3)3·5H2O, obtaining a second mixed solution; wherein the mass ratio of the volume of the ethylene glycol to the PVP is (10-90) mL: (0.5-2.5) g; PVP and Bi (NO)3)3·5H2O、Ti3C2The mass ratio of the powder is 1: (1-5): (0.009-0.04);
mixing the first mixed solution and the second mixed solution, and pre-reacting for 50-120 min (such as 70min) to obtain Ti3C2/Bi2WO6And (3) precursor solution.
In the preparation of Ti3C2/Bi2WO6When the precursor solution is used, the ethylene glycol solution of PVP is adopted for preparing the mixed solution I and the mixed solution IIThe concentration of the liquids was the same.
In one embodiment of the present invention, Ti is prepared3C2/Bi2WO6When the precursor solution is adopted, the ethylene glycol solution of PVP is prepared by a water bath method.
Specifically, the water bath temperature for preparing the ethylene glycol solution of PVP by the water bath method is 80-100 ℃.
In one embodiment of the present invention, Ti is prepared3C2/Bi2WO6And when the precursor solution is used, dropwise adding the mixed solution I into the mixed solution II.
The preparation method of the invention comprises the preparation of Ti3C2/Bi2WO6And (3) a step of a nanosheet array photoelectrode. Wherein Ti is prepared3C2/Bi2WO6The nano-sheet array photoelectrode specifically comprises the following steps:
dipping a conductive substrate into Ti3C2/Bi2WO6Carrying out solvent thermal reaction, cooling and rinsing in the precursor solution, and growing Ti with regular shape on the conductive substrate3C2/Bi2WO6Nanosheet array to obtain Ti3C2/Bi2WO6A nanosheet array. The Ti3C2/Bi2WO6The nano-sheet array can be used as a photoelectrode.
In one embodiment of the present invention, the conductive substrate used comprises one or a combination of two or more of ITO, FTO, carbon cloth, or silicon wafer.
Commercially available conductive substrates. The size of the conductive substrate is not particularly limited and may be selected by those skilled in the art according to actual needs.
In one embodiment of the invention, the conductive substrate is ultrasonically cleaned and then dipped into Ti3C2/Bi2WO6In solution. And ultrasonically cleaning the conductive substrate by using acetone, deionized water and absolute ethyl alcohol respectively, wherein the ultrasonic time is 25-40 min.
In the inventionIn one embodiment, Ti is prepared3C2/Bi2WO6When the nano-sheet array is adopted, the temperature of the solvothermal reaction is 160-200 ℃, and the solvothermal reaction time is 18-32 h.
In one embodiment of the present invention, Ti is prepared3C2/Bi2WO6And when the nano-sheet array is adopted, rinsing is carried out through deionized water and absolute ethyl alcohol.
The preparation method comprises the step of forming Ti by an electrochemical deposition method3C2/Bi2WO6Depositing NiFe-LDH on the nanosheet array to obtain NiFe-LDH/Ti3C2/Bi2WO6And (5) a step of nano sheet array.
In one embodiment of the present invention, the electrochemical deposition process may be a three-electrode system. Wherein, Ti is used3C2/Bi2WO6As a working electrode, a platinum wire was used as a counter electrode and Ag/AgCl was used as a reference electrode.
In one embodiment of the present invention, the deposition voltage of the electrochemical deposition method is-1.0V, and the deposition time is 10s-90 s.
In the preparation method of the invention, Ti is deposited by electrochemical deposition3C2/Bi2WO6When NiFe-LDH is deposited on the nanosheet array, Ti is added3C2/Bi2WO6And (3) dipping the nanosheet array into a NiFe-LDH precursor solution.
Layered Double Hydroxides (LDHs) are Layered inorganic functional materials consisting of positively charged layers and exchangeable interlayer anions.
In a specific embodiment of the present invention, the preparation of the NiFe-LDH precursor solution comprises the following steps:
mixing Ni (NO)3)2·6H2O and FeSO4·7H2Dissolving O in water to obtain a NiFe-LDH precursor solution; wherein Ni (NO)3)2·6H2The concentration of O is 0.05mol/L-0.25 mol/L; FeSO4·7H2The concentration of O is 0.05mol/L-0.25 mol/L.
In one embodiment of the present invention, the NiFe-LDH precursor solution is prepared at N2Is carried out in atmosphere to prevent Fe2+Is oxidized.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The preparation method of the nanosheet array specifically comprises the following steps:
the method comprises the following steps: mixing Ti3AlC2Mixing the powder with HF solution, stirring at room temperature, and etching to remove Ti3AlC2Medium Al layer to obtain Ti3C2；
Step two: centrifugally washing with deionized water, and drying in vacuum to obtain Ti3C2Powder;
step three: preparing ethylene glycol solution of PVP by water bath method, and dissolving Na2WO4·2H2O, obtaining a mixed solution I;
step four: preparing ethylene glycol solution of PVP by water bath method, adding Ti3C2Dispersing the powder in a solution, and dissolving Bi (NO) in the solution3)3·5H2O, obtaining a second mixed solution;
step five: mixing the mixed solution I and the mixed solution II, pre-reacting, and transferring to a high-pressure reaction kettle;
step six: immersing the ultrasonically cleaned conductive substrate into a high-pressure reaction kettle for solvothermal reaction, cooling after the reaction is finished, and rinsing by deionized water and absolute ethyl alcohol to obtain Ti grown on the conductive substrate3C2/Bi2WO6A nanosheet array;
step seven: mixing Ni (NO)3)2·6H2O and FeSO4·7H2Dissolving O in deionized water to obtain electrolyte;
step eight: electrochemical deposition on Ti by means of a three-electrode system3C2/Bi2WO6Depositing NiFe-LDH on the nano sheet array, rinsing with deionized water and naturally oxidizing to obtain NiFe-LDH/Ti3C2/Bi2WO6Ternary composite nanosheet array.
The preparation method of the invention synthesizes Bi through solvothermal synthesis2WO6Nano sheet array simultaneous compounding Ti3C2Compounding NiFe-LDH by electrochemical deposition method to prepare NiFe-LDH/Ti3C2/Bi2WO6The ternary composite nanosheet array can effectively improve the separation efficiency of photon-generated carriers, and simultaneously improve the proportion of {001} crystal face, thereby improving Bi2WO6Photocatalytic activity of the nanosheet array; and NiFe-LDH, Ti3C2As an excellent electrocatalytic material, expandable Bi2WO6The application in photoelectrocatalysis.
The invention also provides a NiFe-LDH/Ti3C2/Bi2WO6Nanosheet array, the NiFe-LDH/Ti3C2/Bi2WO6The nano sheet array is prepared by the preparation method of the invention, and the NiFe-LDH/Ti3C2/Bi2WO6The diameter of the nanosheet array is 100nm-150nm, and the nanosheet array within the diameter range is beneficial to migration and separation of a photon-generated carrier and improves the photoelectric catalytic performance of the photon-generated carrier.
Bi compared with other structures2WO6Ti of the invention3C2/Bi2WO6The nano-sheet array has better effect on photoelectrocatalysis degradation, and Ti3C2/Bi2WO6The nanosheet array being accessible to Ti3C2The photoproduction electron-hole is effectively separated, in addition, photocatalysis and electrocatalysis can be coupled, and the degradation efficiency of pollutants is further improved; ti3C2/Bi2WO6The nano-sheet structure has stronger mechanical strength, is tightly contacted with the conductive substrate and can provide larger surface area in a certain space; ti3C2/Bi2WO6The nano sheet structure belongs to nano magnitude in a certain dimension, and the two-dimensional structure of the nano sheet structure has better transmission performance on photo-generated electrons and holes, so that the carrier mobility can be improved.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The nano-sheet array can be used as a photocatalyst to be applied to photocatalytic reaction, as a photoelectrode to be applied to photoelectric catalytic reaction or as a photoelectric conversion device to be applied to photoelectric devices and solar cells.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The nanosheet array can be particularly used as a photocatalyst for photoelectrocatalytic degradation of a bisphenol A solution. The method specifically comprises the following steps:
with NiFe-LDH/Ti3C2/Bi2WO6The nanosheet array is used as a photo-anode, and the bisphenol A solution is subjected to photoelectrocatalytic degradation by applying a bias voltage of 0-2.5V through an electrochemical workstation.
In one embodiment of the present invention, a solution of bisphenol A as a target contaminant with an initial concentration of 10mg/L is stirred in the dark to physical adsorption equilibrium, and then a 300W xenon lamp is used as a light source to irradiate the light anode with visible light (with a 420nm cut-off filter) with an illumination intensity of 100W/cm2The light source is 15cm away from the quartz reactor; with NiFe-LDH/Ti3C2/Bi2WO6The nano-sheet array is a photo-anode, a bias voltage of 0-2.5V is applied to the bisphenol A solution through an electrochemical workstation to carry out photoelectrocatalysis degradation, and the concentration of the bisphenol A solution is detected by a high performance liquid chromatography; in the process of photoelectrocatalysis degradation, the solution is in a state of continuous magnetic stirring.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The nano-sheet array photocatalyst has high photoelectrocatalysis activity and is pure Bi2WO6Compared with the nanosheet array light, the degradation rate is remarkably improved.
NiFe-LDH/Ti of the invention3C2/Bi2WO6The nano-sheet array has simple manufacturing process and very good repeatability, and is suitable for mass development and production.
NiFe-LDH/Ti prepared by the preparation method of the invention3C2/Bi2WO6The nanosheet array exposes a large proportion of Bi2WO6The {001} crystal face and the {001} crystal face are oxide crystal faces, so that Bi is present2WO6The photocatalyst has higher photocatalytic oxidation performance; by passing Ti3C2The modification of NiFe-LDH effectively promotes the separation and migration of photoproduction electron-hole, thereby greatly improving Bi2WO6The photocatalytic performance of (a); in addition of Ti3C2And NiFe-LDH as excellent electrocatalytic material, and greatly improves Bi2WO6The photocatalytic performance of (a).
Bi in the invention2WO6Bi of nanosheet array compared to other structures2WO6Has better photocatalytic degradation effect, Bi2WO6The nano-sheet array photoelectrode can couple photocatalysis and electrocatalysis, so that the degradation efficiency of pollutants is improved; the nano-sheet structure has stronger mechanical strength, is tightly contacted with the conductive substrate and can provide larger surface area; bi2WO6The nano-sheet structure still belongs to nano-scale in a certain dimension, and the two-dimensional structure of the nano-sheet structure has better transmission performance on photo-generated electrons and holes, so that the carrier mobility can be improved.
NiFe-LDH/Ti of the invention3C2/Bi2WO6Performing photoelectrocatalysis degradation on bisphenol A solution and Ti by taking ternary composite nanosheet array as catalyst3C2Modification with NiFe-LDH improves the separation and utilization efficiency of photo-generated charges; in addition, the separation of an electron reduction process and a hole oxidation process on the space can be further realized through an external bias voltage, the utilization efficiency of a photon-generated carrier is further improved, and the photocatalysis efficiency is further improved.
Drawings
FIG. 1 shows Ti prepared in example 13C2/Bi2WO6Scanning electron microscopy of the nanosheet array.
FIG. 2 shows NiFe-LDH/Ti prepared in example 13C2/Bi2WO6Scanning electron microscopy of the nanosheet array.
FIG. 3 is the NiFe-LDH/Ti prepared in example 13C2/Bi2WO6Nanosheet array and Bi prepared in comparative example 12WO6Nano meterUv-vis diffuse reflectance spectra contrast of the chip array.
FIG. 4 shows NiFe-LDH/Ti prepared in example 13C2/Bi2WO6The nanosheet array serves as a photocatalyst and serves as a degradation curve for the photocatalytic degradation of bisphenol A under the conditions of example 2.
FIG. 5 shows NiFe-LDH/Ti prepared in example 13C2/Bi2WO6The nanosheet array served as a photocatalyst and degraded curve of the photocatalytic degradation of bisphenol a under the conditions of example 3.
FIG. 6 shows Bi prepared in comparative example 12WO6Scanning electron microscopy of the nanosheet array.
FIG. 7 shows Bi prepared in comparative example 12WO6The nanosheet array serves as a photocatalyst and serves as a degradation curve for the photocatalytic degradation of bisphenol A under the conditions of example 2.
FIG. 8 shows Bi prepared in comparative example 12WO6The nanosheet array served as a photocatalyst and photocatalytic degradation bisphenol a degradation profile was obtained under the conditions of example 3.
FIG. 9 shows NiFe-LDH/Ti prepared in example 13C2/Bi2WO6Ternary composite nanosheet array and Bi prepared in comparative example 12WO6Nanoplate arrays as photocatalyst degrade bisphenol a contrast plots under the conditions of example 2 and example 3.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
This example provides a NiFe-LDH/Ti alloy3C2/Bi2WO6The preparation method of the ternary composite nanosheet array photoelectrode specifically comprises the following steps:
the method comprises the following steps: mixing 3g of Ti3AlC2Mixing the powder with 40mL of 40% HF solution, stirring at room temperature for 72h, and etching to remove Ti3AlC2The Al layer in the alloy is Ti3C2；
Step two: washing with deionized water for 5 times at 10000r/min for 15min each time. Subjecting the centrifuged Ti3C2Placing in a vacuum drying oven at 60 deg.C for 24 hr to obtain final Ti3C2A powder sample;
step three: adding 20mL of ethylene glycol into a small beaker, placing the beaker in a water bath at 95 ℃, adding 0.6g of PVP after the temperature of the ethylene glycol reaches 95 ℃, magnetically stirring the mixture until the PVP is completely dissolved, and then adding 0.3299g of Na2WO4·2H2O, magnetically stirring until the O is completely dissolved to obtain a mixed solution I;
step four: adding 20mL of ethylene glycol into a small beaker, placing the beaker in a water bath at 95 ℃, adding 0.6g of PVP after the temperature of the ethylene glycol reaches 95 ℃, magnetically stirring until the PVP is completely dissolved, and then adding Ti3C20.0093g of powder, sealing with preservative film and magnetically stirring to obtain Ti3C2The powder is fully and uniformly dispersed; 0.9701g of Bi (NO) were then added3)3·5H2O, magnetically stirring until the O is completely dissolved to obtain a mixed solution II;
step five: dropwise adding the mixed solution I into the mixed solution II under the condition of continuous magnetic stirring, sealing at 95 ℃, pre-reacting for 60min, and transferring to a 50mL high-pressure reaction kettle;
step six, selecting ITO with the size of 2cm × 3cm as Bi2WO6A growth substrate of the nano-sheet array. And ultrasonically cleaning the ITO in acetone, deionized water and absolute ethyl alcohol for 30min in sequence, and drying by using nitrogen. And then vertically immersing the ITO into the reaction kettle in the sixth step, carrying out solvent thermal reaction for 24 hours at the temperature of 180 ℃, naturally cooling to room temperature, and respectively rinsing with deionized water and absolute ethyl alcohol to obtain Ti-grown Ti3C2/Bi2WO6A photoelectrode of a nanosheet array;
step seven: 70mL of deionized water was added to the cell followed by N2Under the condition of atmosphere and continuously stirring, respectively adding 0.15mol/L of Ni (NO)3)2·6H2O and 0.15mol/L FeSO4·7H2O, obtaining an electrolyte;
step eight: the electrochemical deposition of NiFe-LDH adopts a three-electrode system. Ti3C2/Bi2WO6The photoelectrode, the platinum wire and the Ag/AgCl electrode are respectively used as a working electrode, a counter electrode and a reference electrode, the deposition voltage is-1.0V, and the deposition time is 30 s. Taking out the ITO after the electrochemical deposition is finished, rinsing the ITO with deionized water, and then placing the ITO in the air to enable Fe2+Natural oxidation to Fe3+To obtain NiFe-LDH/Ti3C2/Bi2WO6A nanosheet array.
Ti prepared in this example3C2/Bi2WO6And NiFe-LDH/Ti3C2/Bi2WO6The nanosheet array is subjected to a scanning electron microscope experiment, and the experimental result is shown in fig. 1 and 2, and can be seen from the experimental result in fig. 1 and 2: the Ti3C2/Bi2WO6And NiFe-LDH/Ti3C2/Bi2WO6The diameter of the nano-sheet array is 100nm-150nm, and the appearance is regular.
FIG. 3 shows NiFe-LDH/Ti prepared in this example3C2/Bi2WO6Nanosheet array and Bi prepared in comparative example 12WO6And (3) comparing ultraviolet-visible diffuse reflection spectra of the nanosheet array. As can be seen from fig. 3: bi2WO6The light absorption edge of the nano sheet array is about 425nm, while the NiFe-LDH/Ti3C2/Bi2WO6The light absorption edge of the nano-sheet array is about 450nm, so that Bi is widened2WO6Absorption of visible light.
Example 2
Preparing a solution with bisphenol A as a target pollutant, and carrying out an evaluation experiment of the photoelectrocatalysis degradation activity on the catalyst, wherein the evaluation experiment is carried out according to the following modes:
will grow NiFe-LDH/Ti3C2/Bi2WO6The nano-sheet array is used as a photo-anode and is immersed into bisphenol A solution with the initial concentration of 10mg/L, a standard three-electrode system is adopted, and the photo-anode is applied through an electrochemical workstationA bias voltage of 1.0V;
before the reaction, stirring for a while in dark to allow the photo-anode to reach physical adsorption equilibrium for bisphenol A, and then starting the reaction.
Using 300W xenon lamp as light source, irradiating the light anode with visible light (with 420nm cut-off filter) with illumination intensity of 100W/cm2Sampling every 30min in the degradation process, and storing in dark place; detecting the concentration of the bisphenol A component in the reaction product by high performance liquid chromatography; the bisphenol A solution is always stirred during the reaction.
The NiFe-LDH/Ti prepared in example 1 was subjected to the above-mentioned procedure3C2/Bi2WO6The activity evaluation is carried out by taking the nanosheet array as a photocatalyst, the photoelectrocatalysis reaction is a pseudo-first-order reaction and can pass through ln (C/C)0) Fitting as kt, C0The initial concentration of the solution, C the concentration of the solution at the time of sampling, is denoted as ln (C/C)0) And (3) fitting a data point which changes along with the reaction time t to obtain a straight line of the photoelectrocatalytic degradation bisphenol A solution, wherein the slope of the straight line is an apparent reaction rate constant k of the photoelectrocatalytic degradation reaction, and the slope is shown in figure 4. As is clear from the results in FIG. 4, when the bias was 1.0V, NiFe-LDH/Ti was observed3C2/Bi2WO6The photoelectrocatalysis degradation rate constant k of the nanosheet array is 0.00196min-1Which is about Bi in comparative example 1 described below2WO6The k value of the nanosheet array is 4.5 times. As can be seen, the NiFe-LDH/Ti provided in this example3C2/Bi2WO6The nano-sheet array has high photoelectrocatalysis activity and pure Bi2WO6Compared with a nanosheet array, the degradation rate is remarkably improved.
Example 3
For the NiFe-LDH/Ti prepared in example 13C2/Bi2WO6The activity evaluation of the nanosheet array as a photocatalyst is carried out by the steps similar to those of example 2, but no external bias voltage is applied, so that a straight line of the photocatalytic degradation bisphenol A solution is obtained, as shown in FIG. 5. From the results in FIG. 5, it is clear that NiFe-LDH/Ti3C2/Bi2WO6The photodegradation rate constant k of the nanosheet array was 0.000565min-1Which is Bi in comparative example 1 described below2WO610 times of the nanosheet array. As can be seen, example 1 provides NiFe-LDH/Ti3C2/Bi2WO6The nano-sheet array has high photocatalytic activity and pure Bi2WO6Compared with a nanosheet array, the degradation rate is remarkably improved.
Comparative example 1
This comparative example provides a Bi2WO6The preparation method of the nanosheet array specifically comprises the following steps:
the method comprises the following steps: adding 20mL of ethylene glycol into a small beaker, placing the beaker in a water bath at 95 ℃, adding 0.6g of PVP after the temperature of the ethylene glycol reaches 95 ℃, magnetically stirring the mixture until the PVP is completely dissolved, and then adding 0.3299g of Na2WO4·2H2O, magnetically stirring until the O is completely dissolved to obtain a mixed solution I;
step two: adding 20mL of ethylene glycol into a small beaker, placing the beaker in a water bath at 95 ℃, adding 0.6g of PVP after the temperature of the ethylene glycol reaches 95 ℃, magnetically stirring the mixture until the PVP is completely dissolved, and then adding 0.9701g of Bi (NO)3)3·5H2O, magnetically stirring until the O is completely dissolved to obtain a mixed solution II;
step three: dropwise adding the mixed solution I into the mixed solution II under the condition of continuous magnetic stirring, sealing at 95 ℃, pre-reacting for 60min, and then transferring into a 50mL high-pressure reaction kettle;
step four, selecting ITO with the size of 2cm × 3cm as Bi2WO6A growth substrate of the nano-sheet array. And ultrasonically cleaning the ITO in acetone, deionized water and absolute ethyl alcohol for 30min in sequence, and drying by using nitrogen. Then vertically immersing ITO into the reaction kettle in the third step, carrying out solvent thermal reaction for 24 hours at 180 ℃, naturally cooling to room temperature, and respectively rinsing with deionized water and absolute ethyl alcohol to obtain Bi growing on the ITO2WO6Photoelectrode of nanometer piece array.
Bi prepared for the comparative example2WO6Scanning electron microscope experiment is carried out on the nanosheet array, and the experimental result is shown in figure 6As shown, it can be seen from the experimental results of fig. 6 that: the Bi2WO6The diameter of the nano-sheet array is 150-200nm, and the appearance is regular.
Bi prepared according to comparative example 1 was evaluated according to the method of example 22WO6The nanosheet array was evaluated as a photocatalyst to obtain a curve of photodegraded bisphenol a, as shown in fig. 7. From the results of FIG. 7, it is understood that when the bias voltage is 1.0V, Bi is present2WO6The photoelectric degradation rate constant of the nanosheet array is 0.000438min-1。
Bi prepared in comparative example 1 was added according to the evaluation method of example 32WO6The nanosheet array was evaluated as a photocatalyst to obtain a curve of photodegradable bisphenol a, as shown in fig. 8. From the results in FIG. 8, Bi is shown2WO6The rate constant of photocatalytic degradation of the nanosheet array was 6.47 × 10-5min-1。
The NiFe-LDH/Ti prepared in example 1 was added3C2/Bi2WO6Nanosheet array and Bi prepared in comparative example 12WO6The nanosheet array is used as a photocatalyst for carrying out photoelectrocatalytic degradation and comparison of the photocatalytic degradation bisphenol A, and the experimental result is shown in fig. 9. The corresponding apparent reaction rate constants are shown in Table 1, from which it can be seen that: no matter the photocatalytic degradation or the photoelectrocatalytic degradation, NiFe-LDH/Ti3C2/Bi2WO6Catalytic reaction rate constant k-to-average ratio Bi of nanosheet array2WO6The catalytic reaction rate constant k of the nanosheet array is remarkably improved, which shows that NiFe-LDH and Ti3C2Can effectively improve Bi2WO6The photocatalytic and photoelectrocatalytic activity of the nanosheet array.
TABLE 1 apparent reaction Rate constants of example 1 and comparative example 1
| Photocatalytic degradation | Photoelectrocatalytic degradation | |
| Bi2WO6 | 6.47×10-5min-1 | 0.000438min-1 |
| NiFe-LDH/Ti3C2/Bi2WO6 | 0.000565min-1 | 0.00196min-1 |
The above examples illustrate the production of NiFe-LDH/Ti by the process of the present invention3C2/Bi2WO6The nano-sheet array has good photoelectric catalytic performance, low price, high efficiency and environmental protection.
Claims (10)
1. NiFe-LDH/Ti3C2/Bi2WO6The preparation method of the nanosheet array is characterized by comprising the following steps:
dipping a conductive substrate into Ti3C2/Bi2WO6In the precursor solution, carrying out solvothermal reaction to grow Ti with regular shape on the conductive substrate3C2/Bi2WO6A nanosheet array; the temperature of the solvothermal reaction is 160-200 ℃, and the solvothermal reaction time is 18-32 h;
by electrochemical deposition on Ti3C2/Bi2WO6Depositing NiFe-LDH on the nano sheet array, rinsing and naturally oxidizing to obtain NiFe-LDH/Ti3C2/Bi2WO6A nanosheet array; using Ti in electrochemical deposition3C2/Bi2WO6As a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, the deposition voltage is-1.0V, and the deposition time is 10s-90 s;
the method also includes preparing Ti3C2/Bi2WO6Process for preparing precursor solution, Ti3C2/Bi2WO6The precursor solution comprises the following steps:
adding Na to the ethylene glycol solution of PVP2WO4·2H2O, obtaining a mixed solution I; wherein the mass ratio of the volume of the ethylene glycol to the PVP is (10-90) mL: (0.5-2.5) g; na (Na)2WO4·2H2The mass ratio of O to PVP is 1: (1-5);
adding Ti to a solution of PVP in ethylene glycol3C2Powder of Bi (NO) and re-dissolved3)3·5H2O, obtaining a second mixed solution; wherein the mass ratio of the volume of the ethylene glycol to the PVP is (10-90) mL: (0.5-2.5) g; PVP and Bi (NO)3)3·5H2O、Ti3C2The mass ratio of the powder is 1: (1-5): (0.009-0.04);
mixing the mixed solution I and the mixed solution II, and pre-reacting for 50-120 min to obtain Ti3C2/Bi2WO6Precursor solution;
the method also comprises a process for preparing the NiFe-LDH precursor solution, wherein the process is carried out in the presence of N when the NiFe-LDH precursor solution is prepared2The method is carried out under the atmosphere and comprises the following steps:
mixing Ni (NO)3)2·6H2O and FeSO4·7H2Dissolving O in water to obtain a NiFe-LDH precursor solution; wherein Ni (NO)3)2·6H2The concentration of O is 0.05mol/L-0.25 mol/L; FeSO4·7H2The concentration of O is 0.05mol/L-0.25 mol/L.
2. The method of claim 1, wherein the solution of PVP in ethylene glycol is prepared by a water bath process, wherein the water bath temperature is between 80 ℃ and 100 ℃.
3. The method according to claim 1, wherein the Ti is3C2The powder is prepared by the following steps:
mixing Ti3AlC2Mixing the powder with HF solution, stirring at room temperature for 48-96 h, and etching to remove Ti3AlC2The Al layer in the alloy is Ti3C2(ii) a Wherein, Ti3AlC2The mass ratio of the powder to HF is 1: (5-30);
centrifugally washing and then drying in vacuum to obtain Ti3C2And (3) powder.
4. The method according to claim 3, wherein the concentration of the HF solution is 40wt% to 99 wt%.
5. The method according to claim 3, wherein the rotational speed of the centrifugal washing is 5000 to 10000 r/min; the times of centrifugal washing are 4-8 times; the time of each centrifugation is 5min-30 min.
6. The method of claim 3, wherein the temperature of vacuum drying is 50 ℃ to 100 ℃; the vacuum drying time is 12-48 h.
7. The preparation method according to claim 1, wherein the conductive substrate is one or a combination of two or more of ITO, FTO, carbon cloth or silicon wafer.
8. NiFe-LDH/Ti3C2/Bi2WO6Nanosheet array, characterized in that the NiFe-LDH/Ti3C2/Bi2WO6The nanosheet array is prepared by the preparation method of any one of claims 1 to 7, and the NiFe-LDH/Ti is3C2/Bi2WO6The diameter of the nano-sheet array is 100nm-150 nm.
9. The NiFe-LDH/Ti of claim 83C2/Bi2WO6The application of the nano sheet array is characterized in that the NiFe-LDH/Ti3C2/Bi2WO6The nanosheet array is applied to photocatalytic reaction as a photocatalyst, and is applied to photoelectrocatalysis reaction as a photoelectrode or is applied to photoelectric devices and solar cells as a photoelectric conversion device.
10. Use according to claim 9, wherein said NiFe-LDH/Ti is3C2/Bi2WO6When the nanosheet array is used as a photocatalyst for photoelectrocatalytic degradation of a bisphenol A solution, the method specifically comprises the following steps:
with NiFe-LDH/Ti3C2/Bi2WO6The nanosheet array is used as a photo-anode, and the bisphenol A solution is subjected to photoelectrocatalytic degradation by applying a bias voltage of 1V-2.5V through an electrochemical workstation.
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